CN114575154A - Phase-change energy-storage adhesive and preparation method thereof - Google Patents
Phase-change energy-storage adhesive and preparation method thereof Download PDFInfo
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- CN114575154A CN114575154A CN202210220428.1A CN202210220428A CN114575154A CN 114575154 A CN114575154 A CN 114575154A CN 202210220428 A CN202210220428 A CN 202210220428A CN 114575154 A CN114575154 A CN 114575154A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/04—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention relates to a phase change energy storage viscose fiber and a preparation method thereof. The preparation method comprises the following steps: adding mesoporous silica, a coupling agent and pentaerythritol into water, stirring and cooling to obtain modified pentaerythritol; adding the obtained modified pentaerythritol, benzophenone compounds with alkenyl and benzoyl peroxide into toluene to obtain a mixed solution, carrying out grafting reaction under the atmosphere of inert gas, distilling, cooling, washing and drying; adding the obtained benzophenone modified pentaerythritol and benzoyl peroxide into toluene to obtain a reaction solution; soaking the viscose fiber in water, drying, placing the viscose fiber in a reaction solution under an inert gas atmosphere for grafting reaction, washing and drying to obtain the viscose fiber. According to the invention, the phase-change material pentaerythritol is introduced into the viscose fibers in a grafting manner, so that the bonding strength of the pentaerythritol and the viscose fibers is improved, and the stability of the temperature regulation function of the phase-change energy storage viscose fibers is further improved.
Description
Technical Field
The invention relates to the technical field of household textiles, in particular to a phase change energy storage adhesive and a preparation method thereof.
Background
With the continuous improvement of living standard, functional fibers (such as deodorizing and antibacterial fibers, mosquito repellent fibers, anion fibers and phase change energy storage fibers) and textiles are more and more favored by consumers.
The phase-change energy storage fiber is a heat-storage temperature-regulating fiber developed by utilizing the characteristics that latent heat is released or absorbed in the phase-change process of a substance and the temperature is kept unchanged, and can realize heat exchange with the external environment by utilizing the phase-change process of a phase-change material and keep the temperature of the body relatively constant.
At present, the preparation methods of phase change energy storage fibers or phase change textiles mainly comprise a composite spinning method, a coating method and a hollow fiber dipping method. Wherein, the coating method adopts a coating method to fix the phase change material on the surface of the textile. For example, patent document CN111074366A discloses a process for producing phase change energy storage viscose fiber, which comprises the following steps: preparing a microcapsule emulsion: taking water or alkali liquor as a solvent, adding a dispersing agent into the phase change energy storage microcapsules with the particle size of less than or equal to 2 mu m to prepare microcapsule emulsion with the concentration of 20-40%, and then quantitatively adding desalted water to stir and dilute at the speed of 15-25r/min to obtain microcapsule emulsion with the concentration of 10%; preparing viscose: stopping dissolving the alkali cellulose after yellowing for 50-60 minutes, adding an EBT (ethylene-butyl-phenol) denaturant accounting for 1.5-2.0% of the methyl cellulose, defoaming, filtering and curing to obtain viscose with the content of the methyl cellulose of 7.8-8.5%; preparation of the adhesive crosslinking agent: diluting a certain amount of viscose to the concentration of the alpha-cellulose of 5-6 percent, adding polyacrylamide with the content of the alpha-cellulose of 0.1-0.2 percent, and adding 10 percent hydrogen peroxide with the content of the polyacrylamide of 0.1-0.2 percent to prepare a viscose cross-linking agent; mixing: injecting 10% microcapsule emulsion into viscose together with viscose crosslinking agent at 15-20 deg.C and 0-17Bar temperature and pressure through metering pump at 0.1-0.3m/s speed, and mixing; wherein the weight ratio of the microcapsule emulsion to the viscose cross-linking agent to the viscose is 6-8:1: 100; spinning and post-treatment: and (3) filtering and carrying out acid bath treatment on the mixed product, spinning, and carrying out post-treatment to obtain the phase change energy storage viscose fiber. The microcapsule emulsion, the viscose cross-linking agent and the viscose are mixed under specific temperature, pressure and process parameter ratio, so that the damage rate of the energy storage capsule is effectively reduced, and the utilization rate of the phase change energy storage capsule is improved; the phase change energy storage capsule particles with the average particle size of less than or equal to 2um are used as mixed raw materials, so that the filtering pressure is reduced, the service life of a filter is prolonged, the effective component proportion of the filter in viscose is improved, and the temperature change performance of finished fibers is improved; the polyacrylamide is used as a cross-linking agent to generate intermolecular force with the phase change energy storage capsules and the methyl fibers in the viscose, so that the phase change energy storage capsules and the viscose are highly cross-linked, the energy storage performance of the viscose is ensured after the viscose is formed into filaments, and the high mechanical strength and the high heat resistance are also realized. However, this solution has the following problems: after the fabric processed by the prepared phase change energy storage viscose fiber is washed for many times, the temperature regulation function is obviously reduced.
Disclosure of Invention
In view of the above, the present invention provides a phase change energy storage viscose fiber and a preparation method thereof, which are used to solve the problem that after fabrics processed by the phase change energy storage viscose fiber prepared by the existing method in the prior art are washed for many times, the temperature regulation function is significantly reduced.
In a first aspect, the invention aims to provide a method for preparing a phase change energy storage viscose fiber, which comprises the following steps:
A. adding mesoporous silica, a coupling agent and pentaerythritol into water, stirring, and then cooling to obtain modified pentaerythritol;
B. adding modified pentaerythritol, benzophenone compounds with alkenyl and benzoyl peroxide into toluene to obtain a mixed solution, carrying out grafting reaction in an inert gas atmosphere, distilling, cooling, washing and drying to obtain benzophenone modified pentaerythritol;
C. adding benzophenone modified pentaerythritol and benzoyl peroxide into toluene to obtain a reaction solution; and soaking the viscose fiber in water, drying, then placing the viscose fiber in a reaction solution under an inert gas atmosphere for grafting reaction, and then washing and drying to obtain the phase change energy storage viscose fiber.
In the present invention, the inert gas includes nitrogen, helium, neon, argon, and the like.
Optionally, in step a, the particle size of the mesoporous silica is 50 to 100nm, preferably 50 to 80 nm.
Optionally, in the step a, the mass ratio of the mesoporous silica to the pentaerythritol is 2-3: 1, preferably 2.5 to 3: 1.
optionally, in the step a, the mass ratio of the mesoporous silica to the coupling agent is 100: 0.5-1, preferably 100: 0.6-1.
Optionally, in step a, the coupling agent is selected from a titanate coupling agent or a silane coupling agent.
Optionally, in the step a, the mass ratio of the mesoporous silica to water is 1: 2-5, preferably 1: 3-5.
Optionally, in the step a, the stirring temperature is 150-; the rotating speed of stirring is 150-; the stirring time is 2-3h, preferably 2.5-3 h.
Optionally, in the step B, the mass ratio of the modified pentaerythritol to the benzophenone compound with the alkenyl group is 1: 2-5, preferably 1: 3-5.
Optionally, in step B, the alkenyl benzophenone compound is selected from one or more of 4-propenyloxy-2-hydroxybenzophenone, 4-propenyloxybenzophenone and 3-isopentenyl-2, 4, 6-trihydroxybenzophenone.
Optionally, in the step B, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.1-0.3, preferably 100: 0.2-0.3.
Optionally, in the mixed solution in the step B, the concentration of the modified pentaerythritol is 2 wt% to 5 wt%, preferably 2 wt% to 5 wt%.
Optionally, in step B, the temperature of the grafting reaction is 60-80 ℃, preferably 70-80 ℃; the time of the grafting reaction is 2 to 3 hours, preferably 2.5 to 3 hours.
Optionally, in the step B, the temperature of the distillation is 110-120 ℃, preferably 115-120 ℃.
Optionally, in step B, the drying temperature is 40-50 ℃, preferably 45-50 ℃; the drying time is 10-15h, preferably 12-15 h.
Optionally, in the step C, the mass ratio of the benzophenone-modified pentaerythritol to the benzoyl peroxide is 100: 0.06-0.1, preferably 100: 0.08-0.1.
Optionally, in the reaction solution in step C, the concentration of the benzophenone-modified pentaerythritol is 3 wt% to 7 wt%, preferably 5 wt% to 7 wt%.
Optionally, in step C, the fineness of the viscose fibers is 1 to 3dtex, preferably 1 to 1.5 dtex.
Optionally, in step C, the soaking time is 1.5-3h, preferably 2-3 h.
Optionally, in the soaking process in the step C, the mass ratio of the water to the viscose is 5-10: 1, preferably 8 to 10: 1.
optionally, in step C, the drying temperature is 50-60 ℃, preferably 55-60 ℃; the drying time is 20-30min, preferably 25-30 min.
Optionally, the temperature of the grafting reaction in the step C is 60-80 ℃, preferably 70-80 ℃; the time of the grafting reaction is 2 to 3 hours, preferably 2.5 to 3 hours.
Optionally, in the step C, the drying temperature is 50-60 ℃, preferably 55-60 ℃; the drying time is 20-30min, preferably 25-30 min.
Optionally, azobisisobutyronitrile is further added to the mixed solution in the step B.
Optionally, azobisisobutyronitrile is further added to the reaction solution in the step C.
Optionally, the mass ratio of azobisisobutyronitrile to benzoyl peroxide is 0.5-0.8: 1, preferably 0.6 to 0.8: 1.
optionally, cobalt iso-octoate is further added to the mixed solution in the step B.
Optionally, cobalt iso-octoate is further added into the reaction solution in the step C.
Optionally, the mass ratio of the cobalt isooctanoate to the benzoyl peroxide is 0.2-0.3: 1, preferably 0.25 to 0.3: 1.
optionally, in step C, the mass ratio of the viscose fibers to the reaction solution is 1: 5-10, preferably 8-10: 1.
in a second aspect, the invention also aims to provide the phase change energy storage viscose fiber prepared by the preparation method.
The invention has the beneficial effects that:
(1) according to the invention, through the coupling effect of a titanate coupling agent, the high-thermal-conductivity mesoporous silica and the phase-change material pentaerythritol are coupled together to obtain the modified pentaerythritol, so that the thermal conductivity of the modified pentaerythritol is improved, the temperature regulation function of the modified pentaerythritol is further improved, and a large amount of pentaerythritol can be filled in pores of the mesoporous silica, so that the latent heat of the modified pentaerythritol is improved, and the temperature regulation function of the modified pentaerythritol is further improved; then the modified pentaerythritol is grafted to a benzophenone compound with alkenyl as a photoinitiator under the initiation action of free radicals generated by thermal decomposition of benzoyl peroxide to obtain the benzophenone modified pentaerythritol, and the benzophenone modified pentaerythritol is endowed with a good photocatalytic self-cleaning function; and then, the benzophenone modified pentaerythritol is grafted to the viscose, namely, the phase-change material pentaerythritol is introduced into the viscose in a chemical bond combination mode, so that the combination strength of the pentaerythritol and the cotton fiber is improved, and the temperature regulation function stability of the fabric made of the cotton fiber is improved.
(2) The benzophenone compound with the alkenyl group as the photoinitiator is introduced into the viscose, so that the fabric made of the viscose has a good self-cleaning function; according to the invention, the benzophenone compound with the alkenyl group as the photoinitiator is introduced into the viscose fiber in a chemical bond combination mode rather than a crosslinking mode, so that the bonding strength of the benzophenone compound with the alkenyl group and the viscose fiber is improved, and the stability of the self-cleaning function of the fabric made of the viscose fiber is further improved.
(3) In the invention, water can swell and soften viscose fibers, which is beneficial to the benzoyl peroxide and benzophenone modified pentaerythritol to diffuse and permeate into the fibers, promotes more benzophenone modified pentaerythritol to participate in grafting reaction and promotes the grafting reaction.
(4) According to the invention, the benzoyl peroxide and the azobisisobutyronitrile are compounded for use, so that the half-lives of the benzoyl peroxide and the azobisisobutyronitrile can be adjusted, more benzoyl peroxide and azobisisobutyronitrile are promoted to be decomposed, more free radicals are generated, the grafting reaction is promoted, and the grafting rate is further improved.
(5) In the invention, the cobalt isooctanoate can activate benzoyl peroxide, promote the grafting reaction and further improve the grafting rate.
(6) The phase change energy storage viscose fiber prepared by the invention has good temperature regulation function and self-cleaning performance.
Detailed Description
The present invention is further illustrated by the following specific examples, but it should be noted that the specific material ratios, process conditions, results, etc. described in the examples of the present invention are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the scope of the present invention. It is to be noted that "wt%" as indicated in the description herein means "mass fraction" unless otherwise specified.
The invention provides a preparation method of phase change energy storage viscose fiber, which comprises the following steps:
A. adding mesoporous silica with the particle size of 50-100nm, a coupling agent and pentaerythritol into water, and stirring for 2-3h under the conditions of 150-; the mass ratio of the mesoporous silica to the pentaerythritol is 2-3: 1, the mass ratio of the mesoporous silica to the coupling agent is 100: 0.5-1, wherein the mass ratio of the mesoporous silica to the water is 1: 2-3; then cooling to room temperature to obtain modified pentaerythritol; wherein the coupling agent is selected from titanate coupling agent or silane coupling agent;
B. adding modified pentaerythritol, a benzophenone compound with alkenyl and benzoyl peroxide into toluene to prepare a mixed solution with the concentration of the modified pentaerythritol of 2-5 wt%, wherein the mass ratio of the modified pentaerythritol to the benzophenone compound with alkenyl is 1: 2-5, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.1-0.3; carrying out grafting reaction for 2-3h at the temperature of 60-80 ℃ in the inert gas atmosphere, distilling at the temperature of 100-120 ℃, cooling to room temperature, washing with toluene, and drying at the temperature of 40-50 ℃ for 10-15h to obtain benzophenone modified pentaerythritol; wherein, the benzophenone compound with alkenyl is selected from one or more of 4-propenyloxy-2-hydroxybenzophenone, 4-propenyloxy benzophenone and 3-isopentenyl-2, 4, 6-trihydroxybenzophenone;
C. adding benzophenone modified pentaerythritol and benzoyl peroxide into toluene to prepare a reaction solution with the concentration of the benzophenone modified pentaerythritol of 3 wt% -7 wt%, wherein the mass ratio of the benzophenone modified pentaerythritol to the benzoyl peroxide is 100: 0.06-0.1; placing the viscose fiber with the fineness of 1-3dtex into water with the mass 5-10 times of that of the viscose fiber to be soaked for 1.5-3h, then drying at 50-60 ℃ for 20-30min, then placing the viscose fiber into a reaction solution under the atmosphere of inert gas, carrying out grafting reaction at 60-80 ℃ for 2-3h, then washing with toluene, and drying at 50-60 ℃ for 20-30min to obtain the phase change energy storage viscose fiber.
In another embodiment of the present invention, azobisisobutyronitrile is further added to the mixed solution, wherein the mass ratio of azobisisobutyronitrile to benzoyl peroxide is 0.5-0.8: 1, preferably 0.6 to 0.8: 1.
in another embodiment of the invention, the mixed solution is further added with cobalt iso-octoate, and the mass ratio of the cobalt iso-octoate to the benzoyl peroxide is 0.2-0.3: 1, preferably 0.25 to 0.3: 1.
in another embodiment of the present invention, azobisisobutyronitrile is further added to the reaction solution, wherein the mass ratio of azobisisobutyronitrile to benzoyl peroxide is 0.5-0.8: 1, preferably 0.6 to 0.8: 1.
in another embodiment of the invention, cobalt isooctanoate is further added into the reaction solution, and the mass ratio of the cobalt isooctanoate to the benzoyl peroxide is 0.2-0.3: 1, preferably 0.25 to 0.3: 1.
the present invention will be described in detail below with reference to specific exemplary embodiments. It should also be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention, and that numerous insubstantial modifications and adaptations of the invention described above will occur to those skilled in the art. The specific process parameters and the like of the following examples are also merely one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
A preparation method of phase change energy storage viscose fiber comprises the following specific steps:
A. adding titanate coupling agent TMC-2 into water, stirring, adding mesoporous silicon dioxide and pentaerythritol with the particle size of 50nm, and stirring for 2 hours at 180 ℃ and 180 r/min; then cooling to room temperature to obtain modified pentaerythritol; the mass ratio of the mesoporous silica to the pentaerythritol is 3: 1, the mass ratio of the mesoporous silicon dioxide to the titanate coupling agent TMC-2 is 100: 1, the mass ratio of the mesoporous silica to water is 1: 3;
B. adding modified pentaerythritol, 4-propenyloxy-2-hydroxybenzophenone and benzoyl peroxide into toluene to prepare a mixed solution of the modified pentaerythritol with the concentration of 5 wt%, wherein the mass ratio of the modified pentaerythritol to the 4-propenyloxy-2-hydroxybenzophenone is 1: 5, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.3; carrying out grafting reaction for 2.5h at the temperature of 70 ℃ in the nitrogen atmosphere, distilling at the temperature of 120 ℃, cooling to room temperature, washing with toluene for 3 times, each time for 2min, and drying at the temperature of 45 ℃ for 12h to obtain benzophenone modified pentaerythritol;
C. adding benzophenone modified pentaerythritol and benzoyl peroxide into toluene to prepare a reaction solution with the concentration of the benzophenone modified pentaerythritol of 7 wt%, wherein the mass ratio of the benzophenone modified pentaerythritol to the benzoyl peroxide is 100: 0.1; placing common viscose fiber with the fineness of 1dtex in water with the mass being 8 times of that of the common viscose fiber, soaking for 2 hours, then drying for 25 minutes at the temperature of 55 ℃, then placing the viscose fiber in a reaction solution under the atmosphere of nitrogen, carrying out grafting reaction for 2.5 hours at the temperature of 70 ℃, then washing for 3 times with toluene, each time for 2 minutes, and then drying for 25 minutes at the temperature of 55 ℃ to obtain the phase change energy storage viscose fiber.
Example 2
A preparation method of phase change energy storage viscose fibers comprises the following specific steps:
A. adding a silane coupling agent KH-570 into water, stirring, adding mesoporous silica with the particle size of 8nm and pentaerythritol, and stirring at 170 ℃ and 160r/min for 2.5 h; and then cooling to room temperature to obtain modified pentaerythritol, wherein the mass ratio of the mesoporous silica to the pentaerythritol is 2.5: 1, the mass ratio of the mesoporous silica to the silane coupling agent KH-570 is 100: 0.8, the mass ratio of the mesoporous silica to the water is 1: 2.5;
B. adding modified pentaerythritol, 4-acryloxybenzophenone and benzoyl peroxide into toluene to prepare a mixed solution with the concentration of the modified pentaerythritol of 3 wt%, wherein the mass ratio of the modified pentaerythritol to the 4-acryloxybenzophenone is 1: 4, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.2; carrying out grafting reaction for 2h at the temperature of 80 ℃ in the nitrogen atmosphere, distilling at the temperature of 115 ℃, cooling to room temperature, washing for 2 times with toluene for 3min each time, and drying at the temperature of 50 ℃ for 15h to obtain benzophenone modified pentaerythritol;
C. adding benzophenone modified pentaerythritol and benzoyl peroxide into toluene to prepare a reaction solution with the concentration of the benzophenone modified pentaerythritol of 5 wt%, wherein the mass ratio of the benzophenone modified pentaerythritol to the benzoyl peroxide is 100: 0.08; placing common viscose fiber with the fineness of 1.5dtex into water with the mass of 10 times of that of the common viscose fiber, soaking for 1.5h, then drying for 20min at the temperature of 60 ℃, then placing the viscose fiber into a reaction solution under the nitrogen atmosphere, carrying out grafting reaction for 2h at the temperature of 80 ℃, then washing for 2 times with toluene, 3min each time, and then drying for 20min at the temperature of 60 ℃ to obtain the phase change energy storage viscose fiber.
Example 3
A preparation method of phase change energy storage viscose fibers comprises the following specific steps:
A. adding a silane coupling agent KH-550 into water, then adding mesoporous silica with the particle size of 100nm and pentaerythritol, and stirring for 3 hours at the temperature of 150 ℃ and at the speed of 165 r/min; the mass ratio of the mesoporous silica to the pentaerythritol is 2: 1, the mass ratio of the mesoporous silica to the silane coupling agent KH-550 is 100: 0.5, the mass ratio of the mesoporous silica to the water is 1: 2; then cooling to room temperature to obtain modified pentaerythritol;
B. adding modified pentaerythritol, 3-isopentenyl-2, 4, 6-trihydroxybenzophenone and benzoyl peroxide into toluene to prepare a mixed solution with the concentration of the modified pentaerythritol of 2 wt%, wherein the mass ratio of the modified pentaerythritol to the 3-isopentenyl-2, 4, 6-trihydroxybenzophenone is 1: 2, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.1; carrying out grafting reaction for 3h at the temperature of 60 ℃ in the nitrogen atmosphere, distilling at the temperature of 100 ℃, cooling to room temperature, washing for 3 times with toluene for 2min each time, and drying at the temperature of 40 ℃ for 10h to obtain benzophenone modified pentaerythritol;
C. adding benzophenone modified pentaerythritol and benzoyl peroxide into toluene to prepare a reaction solution with the concentration of the benzophenone modified pentaerythritol of 3 wt%, wherein the mass ratio of the benzophenone modified pentaerythritol to the benzoyl peroxide is 100: 0.06; placing common viscose fiber with the fineness of 3dtex in water with the mass 5 times of that of the common viscose fiber, soaking for 3 hours, then drying for 30 minutes at the temperature of 50 ℃, then placing the viscose fiber in a reaction solution under the nitrogen atmosphere to perform grafting reaction for 3 hours at the temperature of 60 ℃, then washing for 3 times with toluene for 2 minutes each time, and then drying for 30 minutes at the temperature of 50 ℃ to obtain the phase change energy storage viscose fiber.
Example 4
A phase change energy storage viscose fiber was prepared in the same manner as in example 1, except that the following conditions were applied:
B. adding modified pentaerythritol, 4-propenyloxy-2-hydroxybenzophenone, benzoyl peroxide and azobisisobutyronitrile into toluene, stirring at 180 ℃ for 2 hours at a speed of 180r/min to prepare a mixed solution of the modified pentaerythritol with the concentration of 2 wt%, wherein the mass ratio of the modified pentaerythritol to the 4-propenyloxy-2-hydroxybenzophenone is 1: 2, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.1, the mass ratio of the azodiisobutyronitrile to the benzoyl peroxide is 0.8: 1; and carrying out grafting reaction for 3h at the temperature of 60 ℃ in a nitrogen atmosphere, distilling at the temperature of 120 ℃, then cooling to room temperature, washing for 3 times with toluene for 2min each time, and then drying at the temperature of 40 ℃ for 12h to obtain the benzophenone modified pentaerythritol.
Example 5
A phase change energy storage viscose fiber was prepared in the same manner as in example 1, except for the following conditions:
C. adding benzophenone modified pentaerythritol, benzoyl peroxide and azobisisobutyronitrile into toluene to prepare a reaction solution with the concentration of the benzophenone modified pentaerythritol of 5 wt%, wherein the mass ratio of the benzophenone modified pentaerythritol to the benzoyl peroxide is 100: 0.08, the mass ratio of the azodiisobutyronitrile to the benzoyl peroxide is 0.5: 1; soaking the viscose in water with the mass 10 times of that of the viscose for 1.5h, then drying at 60 ℃ for 20min, then placing the common viscose with the fineness of 1dtex in a reaction solution under the nitrogen atmosphere, carrying out grafting reaction at 80 ℃ for 2h, then washing with toluene for 3 times, 2min each time, and then drying at 60 ℃ for 20min to obtain the phase change energy storage viscose.
Example 6
A phase change energy storage viscose fiber was prepared in the same manner as in example 1, except that the following conditions were applied:
B. adding cobalt iso-octoate into toluene, stirring, adding modified pentaerythritol, 4-propylene oxy-2-hydroxybenzophenone and benzoyl peroxide, stirring for 2 hours at 180 ℃ and 180r/min, and preparing a mixed solution of the modified pentaerythritol with the concentration of 5 wt%, wherein the mass ratio of the modified pentaerythritol to the 4-propylene oxy-2-hydroxybenzophenone is 1: 5, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.3, the mass ratio of the cobalt isooctanoate to the benzoyl peroxide is 0.3: 1; and carrying out grafting reaction for 2.5h at the temperature of 70 ℃ in a nitrogen atmosphere, distilling at the temperature of 120 ℃, then cooling to room temperature, washing with toluene for 3 times of 2min each time, and then drying at the temperature of 45 ℃ for 12h to obtain the benzophenone modified pentaerythritol.
Example 7
A phase change energy storage viscose fiber was prepared in the same manner as in example 1, except for the following conditions:
C. adding cobalt isooctanoate into toluene, stirring, adding benzophenone modified pentaerythritol and benzoyl peroxide to prepare a reaction solution with the concentration of the benzophenone modified pentaerythritol of 7 wt%, wherein the mass ratio of the benzophenone modified pentaerythritol to the benzoyl peroxide is 100: 0.1, the mass ratio of the cobalt isooctanoate to the benzoyl peroxide is 0.2: 1; soaking the viscose in water with the mass of 8 times of that of the viscose for 2 hours, then drying the viscose for 25 minutes at the temperature of 55 ℃, then placing the common viscose with the fineness of 1dtex in a reaction solution under the nitrogen atmosphere, carrying out grafting reaction for 2.5 hours at the temperature of 70 ℃, then washing the viscose for 3 times with toluene for 2 minutes each time, and then drying the viscose for 25 minutes at the temperature of 55 ℃ to obtain the phase change energy storage viscose.
Comparative example 1
Common viscose fibres of the same fineness of 1dtex as the source of example 1.
Performance detection
Respectively processing the phase change energy storage viscose fibers prepared in the embodiments 1 to 7 and the viscose fiber prepared in the comparative example 1 into fabrics, taking 500mm by 500mm samples, detecting the thermal resistance of the samples according to the determination of thermal resistance and wet resistance (evaporation heating plate method) of GB/T11048-;
then the fabric is washed 20 times according to the test condition AIM of GB/T12490 + 1990 test method for color fastness to household and commercial washing, ECE standard detergent is adopted, each washing is equivalent to 5 times of washing (namely equivalent to 50 times of washing in total), and the specific washing conditions are as follows: washing with 150mL solution and 10 steel balls at 40 ℃ for 45min, taking out a sample after washing, and washing twice in 100mL water at 40 ℃ for 1min each time; after cleaning, fully cleaning the sample by using water, and airing;
the thermal resistance of the sample is detected again according to the measurement of thermal resistance and wet resistance (evaporation heating plate method) under the steady-state condition of the physiological comfort of the textile GB/T11048 and 2018, the result is shown in Table 1, and the formula is adopted
Calculating the heat transfer coefficient retention rate of the sample before and after cleaning, and the result is shown in table 1; in the formula, gammaFront sideTo determine the thermal resistance of the sample before cleaning,unit is m2·K/W；γRear endThermal resistance of the cleaned sample in m2K/W; lambda is the heat transfer coefficient retention rate, and the unit is%;
detecting the acetaldehyde photocatalytic removal rate of the sample according to GB/T23761-2009 photocatalytic air purification material performance test method, and according to a formula
The photocatalytic removal function retention rate of acetaldehyde in the sample was calculated, and the result is shown in Table 1, wherein ω isFront sideThe unit is the acetaldehyde photocatalytic removal rate of the sample before cleaning; omegaRear endThe unit is the acetaldehyde photocatalytic removal rate of the sample before cleaning; eta is the photocatalytic removal function retention rate of acetaldehyde in the sample, and the unit is percent.
TABLE 1 Performance test results
| Source | γFront part/(m2·K/W) | γRear end/(m2·K/W) | λ/％ | ωFront side/％ | ωRear end/％ | η/％ |
| Example 1 | 0.32 | 0.34 | 94.12 | 61 | 58 | 95.08 |
| Example 2 | 0.34 | 0.37 | 91.89 | 58 | 57 | 98.28 |
| Example 3 | 0.37 | 0.40 | 92.5 | 52 | 50 | 96.15 |
| Example 4 | 0.26 | 0.27 | 96.30 | 70 | 67 | 95.71 |
| Example 5 | 0.28 | 0.29 | 96.55 | 67 | 66 | 98.51 |
| Example 6 | 0.25 | 0.27 | 92.59 | 72 | 70 | 97.22 |
| Example 7 | 0.26 | 0.27 | 96.30 | 69 | 68 | 95.55 |
| Comparative example 1 | 0.43 | 0.44 | 97.73 | 0 | 0 | -- |
As can be seen from table 1, the heat transfer coefficient retention rate of the fabrics processed from the phase change energy storage viscose fibers of examples 1 to 7 is up to 90% or more before and after cleaning, and the acetaldehyde photocatalytic removal performance retention rate is up to 95% or more, which indicates that the phase change energy storage fibers of the present invention have good temperature regulation function and good stability of the photocatalytic self-cleaning function.
As can be seen from table 1, compared with comparative example 1, the thermal resistance of the fabrics (the samples before cleaning) processed by the phase change energy storage viscose fibers of examples 1 to 7 is significantly reduced, and the results show that the phase change energy storage fibers of the present invention have a good temperature transmission regulating function.
Compared with the sample before cleaning in the example 1, the thermal resistance of the fabric (sample before cleaning) processed by the phase change energy storage fiber in the example 1 is reduced by about 25.6 percent.
Compared with the sample before cleaning in the example 1, the thermal resistance of the fabrics (sample before cleaning) processed by the phase change energy storage fibers in the example 4 and the example 5 is reduced by about 18.8 percent and 12.5 percent respectively.
The thermal resistance of the fabrics (pre-cleaning samples) processed from the phase change energy storage fibers of example 6 and example 7 was reduced by about 21.9% and about 18.8% compared to example 1 (pre-cleaning samples), respectively.
In conclusion, the invention effectively improves the bonding fastness of the phase-change material pentaerythritol and the photoinitiator 4-propylene oxy-2-hydroxybenzophenone with the viscose fiber, and further improves the temperature regulation function and the stability of the photocatalytic self-cleaning function of the fabric processed by the phase-change energy-storage viscose fiber.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. The preparation method of the phase-change energy-storage viscose fiber is characterized by comprising the following steps of:
A. adding mesoporous silica, a coupling agent and pentaerythritol into water, stirring, and then cooling to obtain modified pentaerythritol;
B. adding modified pentaerythritol, benzophenone compounds with alkenyl and benzoyl peroxide into toluene to obtain a mixed solution, carrying out grafting reaction in an inert gas atmosphere, distilling, cooling, washing and drying to obtain benzophenone modified pentaerythritol;
C. adding benzophenone modified pentaerythritol and benzoyl peroxide into toluene to obtain a reaction solution; and soaking the viscose fiber in water, drying, then placing the viscose fiber in a reaction solution under an inert gas atmosphere for grafting reaction, and then washing and drying to obtain the phase change energy storage viscose fiber.
2. The preparation method according to claim 1, wherein in the step a, the particle size of the mesoporous silica is 50 to 100 nm;
and/or in the step A, the mass ratio of the mesoporous silica to the pentaerythritol is 2-3: 1;
and/or in the step A, the mass ratio of the mesoporous silica to the coupling agent is 100: 0.5 to 1;
and/or, in step A, the coupling agent is selected from titanate coupling agent or silane coupling agent;
and/or in the step A, the mass ratio of the mesoporous silica to the water is 1: 2-5;
and/or in the step A, the stirring temperature is 150-.
3. The method according to claim 1, wherein in step B, the mass ratio of the modified pentaerythritol to the alkenyl benzophenone compound is 1: 2-5;
and/or, in the step B, the benzophenone compound with the alkenyl group is selected from one or more of 4-propenyloxy-2-hydroxybenzophenone, 4-propenyloxy benzophenone and 3-isopentenyl-2, 4, 6-trihydroxybenzophenone;
and/or in the step B, the mass ratio of the modified pentaerythritol to the benzoyl peroxide is 100: 0.1-0.3;
and/or in the mixed solution in the step B, the concentration of the modified pentaerythritol is 2-5 wt%;
and/or in the step B, the temperature of the grafting reaction is 60-80 ℃, and the time of the grafting reaction is 2-3 h;
and/or, in the step B, the temperature of the distillation is 110-120 ℃, preferably 112-120 ℃; and/or in the step B, the drying temperature is 40-50 ℃, and the drying time is 10-15 min.
4. The preparation method according to claim 1, wherein in step C, the mass ratio of the benzophenone-modified pentaerythritol to the benzoyl peroxide is 100: 0.06-0.1;
and/or, in the reaction solution in the step C, the concentration of the benzophenone modified pentaerythritol is 3 wt% to 7 wt%;
and/or in the step C, the fineness of the viscose fiber is 1-3 dtex;
and/or, in the step C, the soaking time is 1.5-3 h;
and/or in the soaking process in the step C, the mass ratio of the water to the viscose fibers is 5-10: 1;
and/or in the step C, the drying temperature is 50-60 ℃, and the drying time is 20-30 min;
and/or in the step C, the temperature of the grafting reaction is 60-80 ℃, and the time of the grafting reaction is 2-3 h;
and/or in the step C, the drying temperature is 50-60 ℃, and the drying time is 20-30 min.
5. The method according to claim 1, wherein azobisisobutyronitrile is further added to the mixed solution of step B;
and/or azodiisobutyronitrile is further added into the reaction solution in the step C.
6. The method according to claim 5, wherein the mass ratio of azobisisobutyronitrile to benzoyl peroxide is 0.5 to 0.8: 1.
7. the method according to claim 1, wherein cobalt iso-octoate is further added to the mixed solution in the step B;
and/or, adding cobalt isooctanoate into the reaction solution in the step C.
8. The method according to claim 7, wherein the mass ratio of the cobalt isooctanoate to the benzoyl peroxide is 0.2-0.3: 1.
9. the preparation method according to claim 1, wherein in the step C, the mass ratio of the viscose fiber to the reaction solution is 1: 5-10.
10. The phase change energy storage viscose fiber prepared by the preparation method according to any one of claims 1 to 9.
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| US4851291A (en) * | 1986-06-19 | 1989-07-25 | The United States Of America As Represented By The Secretary Of Agriculture | Temperature adaptable textile fibers and method of preparing same |
| CN1908258A (en) * | 2006-08-10 | 2007-02-07 | 中国科学院广州化学研究所 | Phase-change energy-storage ultra-fine composite fiber and preparation method and application thereof |
| US20070089276A1 (en) * | 2005-09-15 | 2007-04-26 | Fiber Innovation Technology, Inc. | Multicomponent fiber comprising a phase change material |
| CN108360080A (en) * | 2018-02-12 | 2018-08-03 | 天津工业大学 | A kind of cellulose-acrylate base solid-solid phase transition material and preparation method thereof |
| CN111705509A (en) * | 2020-07-08 | 2020-09-25 | 南京轮廓服饰科技有限公司 | Graphene-based lasting antibacterial composite garment fabric |
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|---|---|---|---|---|
| US4851291A (en) * | 1986-06-19 | 1989-07-25 | The United States Of America As Represented By The Secretary Of Agriculture | Temperature adaptable textile fibers and method of preparing same |
| US20070089276A1 (en) * | 2005-09-15 | 2007-04-26 | Fiber Innovation Technology, Inc. | Multicomponent fiber comprising a phase change material |
| CN1908258A (en) * | 2006-08-10 | 2007-02-07 | 中国科学院广州化学研究所 | Phase-change energy-storage ultra-fine composite fiber and preparation method and application thereof |
| CN108360080A (en) * | 2018-02-12 | 2018-08-03 | 天津工业大学 | A kind of cellulose-acrylate base solid-solid phase transition material and preparation method thereof |
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